顶空气相色谱法测定注射用胸腺法新中5种有机溶剂残留量  

Determination of residues of five organic solvents in thymalfasin for injection by HS-GC

作　　者：张洁 程龙 陈霞 ZHANG Jie;CHENG Long;CHEN Xia(Chengdu institute for Drug Control,Chengdu 610041,China)

机构地区：[1]成都市药品检验研究院,四川成都610041

出　　处：《药物评价研究》2022年第3期500-503,共4页Drug Evaluation Research

基　　金：四川省科技计划项目:高端制剂共性关键技术研究与公共技术服务示范基地建设(2020YFS0570)。

摘　　要：目的 建立同时测定注射用胸腺法新中乙腈、二氯甲烷、醋酸乙酯、苯和苯甲醚5种有机溶剂残留量的顶空气相色谱法。方法 采用Agilent DB-624(30 m×0.53 mm×3μm)毛细管色谱柱;火焰离子化检测器;进样口温度200℃;检测器温度250℃;载气为氮气;载气体积流量为2.0 mL·min^(-1);分流比为10∶1;升温程序:起始温度40℃,保持6 min,以8℃·min^(-1)的速率升温至90℃,保持2 min,再以20℃·min^(-1)的速率升温至200℃,保持5 min;采用顶空进样方式,顶空加热箱温度80℃,样品瓶平衡时间30 min。进行系统适用性、检测限(LOD)与定量限(LOQ)、线性关系和范围、加样回收率、精密度、稳定性、耐用性考察。结果 注射用胸腺法新中5种残留溶剂在各自线性浓度范围内与峰面积线性关系良好;平均加样回收率在95.7%~106.3%;精密度、稳定性、耐用性均符合要求。5批胸腺法新中均未检出5种有机溶剂。结论建立的顶空气相色谱法操作简单、灵敏度和准确度高、重现性和耐用性好,可用于注射用胸腺法新中5种有机溶剂残留量的测定。Objective To establish HS-GC method to simultaneously determine the residues of five organic solvents(acetonitrile,dichloromethane,ethyl acetate,benzene,and anisole) in thymalfasin for injection.Methods The determination was performed on Agilent DB-624 capillary column(30 m × 0.53 mm × 3 μm) with temperature programming by FID.The inlet temperature was200 ℃ and the detector temperature was 250 ℃.The carrier gas was nitrogen,and the carrier gas flow rate was 2 mL·min^(-1).The column temperature started at 40 ℃ for 6 min,and then at 8 ℃·min^(-1) to 90 ℃ for 2 min,followed by 20 ℃·min^(-1) to 200 ℃ for 5 min.The temperature of HS heating box was 80 ℃ and the equilibrium time of sample bottle was 30 min.Results The five residual solvents in thymalfasin for injection had a good linear relationship in their concentration ranges(r > 0.999).The average recovery was 95.7%—106.3%.Precision,stability and durability all meet the requirements.Conclusion The method is simple,sensitive,accurate,reproducible and durable,and can be used to determine the residues of five organic solvents in thymalfasin for injection.

关 键 词：注射用胸腺法新 溶剂残留 顶空气相色谱法 乙腈 二氯甲烷 醋酸乙酯 苯 苯甲醚 

分 类 号：R917[医药卫生—药物分析学]